The selenium content of a variety of food items representing a normal hospital diet has been determined by cyclic instrumental neutron activation analysis (CINAA) through the 162-keV gamma-ray of the77mSe nuclide. The CINAA method is very simple and rapid. It involves irradiation of a sample for 20 s, decay for 20 s, and counting for 20 s. The precision of the method has been significantly improved by recycling the samples up to 4 times. The accuracy has been evaluated by analyzing a number of certified reference materials of varied selenium levels.
The comparability of analytical results from different laboratories requires accurately known concentrations in the applied standards. Dilution effects of different multielement synthetic standard solutions have been studied by measuring 10–12 different concentrations of the same solution. Peak area comparison of four Certified Reference Materials (CRM's) using one value for the evaluation of the other three repetitively led to the intercomparison (degree of compatibility) of the certified values. The idea of the preparation of each laboratory's secondary reference standard by comparison of synthetic multielement standards with as many CRM's as practically feasible is advocated to improve the reliability of analytical results.
Authors:G. Wauters, C. Vandecasteele, K. Strijckmans, and J. Hoste
Cadmium, thallium and lead are determined in environmental samples using the111,112,113Cd(p,xn)111In,203Tl(p,3n)201Pb and206,207,208Pb(p,xn)206Bi reactions.111In.201Pb and206Bi are chemically separated by anion exchange and anodic deposition of lead(IV). oxide. Detection limits are 6, 44 and 25 ng/g for cadmium, thallium and lead, respectively. The results obtained for certified reference materials are in good agreement with the certified values.
Authors:S. Heller-Zeisler, M. Donais, and R. Zeisler
Instrumental neutron activation analysis (INAA) has been employed in the investigation of mass balance for mercury species
analysis in the analytical process. A new human hair reference material (IAEA-085) was analyzed for methylmercury using a
solid/liquid extraction procedure, with samples of extracts, residues, and untreated samples being analyzed by INAA. The certified
reference material NIES CRM No. 13, human hair, was analyzed in parallel. From the results obtained through the mass balance
studies, it was found that the extraction procedure was quantitatively complete, and that there was no difference between
the mass balance of Hg and the total Hg in the untreated materials.
Instrumental neutron activation analysis was used to determine selenium concentrations in several marine organisms including two certified reference materials /NRCC lobster hepatopancreas, NBS oyster tissue/ and one uncertified material /IAEA fish homogenate/. The76Se/n, /77mSe/T=17.4 s/ reaction was successfully employed to achieve an overall precision between 3–10% and detection limits between 0.3–0.6 g/g. The accuracy of the results, as compared to the certified values, was in excellent agreement with the NBS material and only slightly lower /9%/ for the NRCC material.
Authors:G. Arana, U. Wätjen, C. Ingelbrecht, and P. Robouch
Five copper alloys were prepared with modern powder metallurgical processes in the frame of the European project Improvement of Means of Measurement on Archaeological Copper-Alloys for Characterisation and Conservation (IMMACO) and certified for As, Pb, Sn and Zn mass fractions. Similar in their composition to archaeological bronze alloys, these Certified Reference Materials (CRMs) are to be used for calibration of XRF instruments for characterization of archaeological samples either in the laboratory or in the field. This paper presents and compares the successful contribution of our non-destructive analytical methods (k0-NAA and PIXE) to the IMMACO project and to the certification of the five reference materials.
Authors:A. Kimura, Y. Toh, M. Oshima, Y. Hatsukawa, and J. Goto
Recycled steel products demands a new technique for determining tramp elements in steel. In this paper, As and Sb in iron
certified reference materials were determined by neutron activation analysis with the multiple gamma-ray detection method.
The determined values are in good agreement with certified and reference values. The lower determination limits (LDL) for
As and Sb in high purity iron are 0.012 and 0.0025 ppm, respectively. As the demanded LDL for As and Sb is 0.1 ppm, the method
described in this work is suitable for determining As and Sb in recycled steel.
Authors:M. Bacchi, L. Santos, E. De Nadai Fernandes, P. Bode, F. Tagliaferro, and E. França
The effectiveness of a Compton suppression system (CSS) for instrumental neutron activation analysis of plant materials was
evaluated. Suppression factors were measured with 137Cs sources. Five certified reference materials were analyzed and the detection limits calculated from both suppressed and
unsuppressed spectra were compared. The CSS demonstrated to be useful for lowering the detection limits of ten out of sixteen
elements tested, showing a maximum improvement factor of 3.9. The system performance was strongly influenced by the sample
composition and also by the measurement conditions, indicating the importance of testing each individual sample type and analytical
The thermal neutron prompt gamma-ray activation analysis (PGAA) facility, operated by the US Food and Drug Administration and National Institute of Standards and Technology Center for Neutron Research, has been redesigned to lower background radiation levels and improved analytical capabilities. Analysis of 22 element standards and food and botanical certified reference materials revealed significant sensitivity increases and lower limits of detection for H, B, C, N, Na, Al, P, S, Cl, K, Ca, Fe, and Cd. Mass fractions for these elements, as well as Mg, Al, Si, Ti, Mn, Fe, Cu, I, Zn, Sm, and Gd, were determined for 6 dietary supplements.
A fast pneumatic transfer facility was installed in Nuclear Engineering Teaching Laboratory (NETL) of the University of Texas
at Austin for the purpose of cyclic thermal and epithermal neutron activation analysis. In this study efforts were focused
on the evaluation of cyclic epithermal neutron activation analysis (CENAA). Various NIST and CANMET certified materials were
analyzed by the system. Experiment results showed 110Ag with its 25 s half-life as one of the isotopes favored by the system. Thus, the system was put into practical application
in identifying silver in metallic ores. Comparison of sliver concentrations as determined by CENAA in CANMET certified reference
materials gave very good results.